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Herein, we presented a self\u2010standing covalent organic framework (COF) membrane formed between 1,3,5\u2010tris\u2010(4\u2010aminophenyl)triazine (TTPA) and 4,4',4''\u2010nitrilotribenzaldehyde (TFPA), TTPA\u2013TFPA COF, which was fabricated via a two\u2010step synthesis involving interface\u2010confined polymerization followed by post\u2010processing. The sensor used the ozone\u2010treated COF membrane as the sensing layer exhibited rapid, highly selective, and visually observable fluorescence response toward the NPS simulant (S)\u2010\n                    <jats:italic>N<\/jats:italic>\n                    ,\n                    <jats:italic>\u03b1<\/jats:italic>\n                    \u2010dimethylbenzylamine (DMBA), achieving a fast response time of less than 1\u00a0min and an ultra\u2010low detection limit of 2.1 ppb. Moreover, the sensor successfully discriminates seven structurally analogous NPS reference standards through kinetic response profiling. The infrared and XPS spectra, along with theoretical calculations, further reveal the sensing mechanism is driven by hydrogen bond interaction between the ozone\u2010treated COF membrane and the DMBA. These findings offer valuable insights for developing portable, real\u2010time chemical monitoring devices, providing an innovative solution for on\u2010site trace\u2010level NPS detection. This holds promising potential for addressing serious threats to human health, family harmony, and social stability.\n                  <\/jats:p>","DOI":"10.1002\/anie.5244392","type":"journal-article","created":{"date-parts":[[2026,4,17]],"date-time":"2026-04-17T05:44:59Z","timestamp":1776404699000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":3,"title":["Protonation\u2010Triggered Fluorescence Switching in COF Membranes for the Selective and Rapid Detection of New Psychoactive Substances"],"prefix":"10.1002","volume":"65","author":[{"given":"Yan","family":"Luo","sequence":"first","affiliation":[{"name":"Key Laboratory of Applied Surface and Colloid Chemistry Ministry of Education Shaanxi Provincial Key Laboratory of New Concept Sensors and Molecular Materials School of Chemistry and Chemical Engineering Shaanxi Normal University  Xi'an P. R. 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